This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D 1514 – 001
Standard Test Method for
Carbon Black—Sieve Residue1
This standard is issued under the fixed designation D 1514; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method describes the determination of the water wash sieve residue in regular untreated carbon blacks. It may not
be applicable to oil-treated carbon blacks because the oil would prevent proper wetting of the black by water.
1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. For specific precautionary statements, see Section 6.
2. Referenced Documents
2.1 ASTM Standards:
1
This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon Black
Components of Carbon Black.
Current edition approved May Dec. 10, 20001. Published July 2000. February 2002. Originally published as D 1514 – 57 T. Last previous edition D 1514 – 9900.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
D 1514 – 001
D 1799 Practice for Carbon Black—Sampling Packaged Shipments2
D 1900 Practice for Carbon Black—Sampling Bulk Shipments2
D 4483 Practice for Determining Precision for Test Method Standards in the Rubber and Carbon Black Industries2
E 11 Specification for Wire- Cloth and Sieves for Testing Purposes3
3. Summary of Test Method
3.1 A sample of carbon black is washed with water through a wire mesh screen of a specified size until all that remains is a
non-carbon black residue. This residue is dried, weighed, and the amount of residue is expressed as mg/kg (ppm) of the original
sample.
4. Significance and Use
4.1 The quantity of sieve residue of carbon black is important in some molded or extruded products as it may relate to the
surface appearance of those products. The maximum residue in each application is normally determined and agreed to between
the user and the producer.
5. Apparatus
5.1 Sieve and Filtering Apparatus, 4 as shown in Fig. 1.
5.2 Balance, with a sensitivity of 0.01 g.
5.3 Analytical Balance, with a sensitivity of 0.1 mg.
5.4 Oven, gravity-convection type, capable of temperature regulation within 61°C at 125°C and temperature uniformity within
65°C.
5.5 Sieves of either phosphor bronze or stainless steel. The sieve shall conform to be in accordance with Specification E 11. The
sieve to be used shall be agreed upon between the purchaser and the seller.
2
Annual Book of ASTM Standards, Vol 09.01.
Annual Book of ASTM Standards, Vol 14.02.
4
Sieve and filtering apparatus, available from Titan Specialties, Inc., P.O. Box 2316, Pampa, TX 70066-2316, has been found suitable. The A2000 Test Set from Krahnen
IQS, GmbH, Paffrather Str. 13–15, D-51069 Koeln, Germany, has been found suitable. An ASTM specified apparatus modified with an enlarged funnel leg ID (5.080 cm or
2.0 in.) and sieve screen OD (6.032 cm or 2.375 in.) has also been found suitable.
3
NOTE 1—Industrial/O.E.M. filter and pleated polyester fabric reusable
cartridges have been found to be a satisfactory strainer. Housing No. 20
and cartridge No. 30 are available from Amtec, Plymouth Products
Division, 562 Indiana Ave., Sheboygan, WI 53081.
NOTE 2—Corrosion-free piping must be used.
NOTE 3—Detailed drawings can be obtained from Test Method
D 1514 – 88a.
NOTE 4—Spray nozzle: Part No. 460.746.30 BE available from Lechler
Inc., 445 Kautz Rd., St. Charles, IL 60174, or Titan Specialties Inc., P.O.
Box 2316, Pampa, TX 70066-2316.
FIG. 1 Schematic Diagram of Apparatus for Sieve Residue
Determination
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D 1514 – 001
5.6 Weighing Dishes.
6. Precautions
6.1 Keep the apparatus clean at all times to prevent contamination.
6.2 Examine the sieves each time they are used to make sure that no cracks or holes have developed.
6.3 Examine the strainer periodically to ascertain that the filter screen is in good condition.
7. Sampling
7.1 Samples shall be taken in accordance with Practice D 1799 or Practice D 1900.
8. Calibration
8.1 Calculate the sieve residue to the nearest mg/kg (ppm) as follows:
R 5 ~W/S! 3 10 6
(1)
where:
R = sieve residue, mg/kg (ppm),
W = mass of sieve residue, g, and
S = mass of sample, g.
9. Procedure
9.1 Prior to making a test, clean the strainer by opening valves A and B and closing valve C as shown in Fig. 1. Allow the strainer
to wash for 2 min.
9.2 Close valve B and open valve C. With valves A and C completely open, regulate the water pressure by means of a reducing
valve. The recommended water pressure is 207 6 34 kPa (30 6 5 lbf/in.2).
9.3 After the water pressure has been regulated, attach the sieve holder with a 50 mm (2 in.) diameter sieve to the funnel and
allow the water to run through it for 3 min. Stop the water flow by closing valves A and C. Examine the sieve for particles; if none
are observed, the apparatus is ready for use.
9.4 Weigh 100.0 g of the carbon black on the balance.
9.5 Attach the proper sieve to the funnel and start the water flow by opening valves A and C.
9.6 Add the carbon black slowly to the funnel to prevent plugging of the sieve.
NOTE 1—If desired, it shall be permissible to disperse the carbon black in water using a high speed stirring apparatus. It shall also be permissible to
utilize wetting agents to facilitate dispersion. Care must be taken to ensure that all of the solid material is transferred from the vessel used for dispersing
the black into the funnel of the washing apparatus.
9.7 Use a gentle stream of water from the hose attached to valve D to wash down any carbon black on the sides of the funnel.
9.8 Continue washing until the wash water coming through the sieve is clear.
9.9 Remove the sieve holder and sieve from the funnel and rub the residue lightly with the finger to disaggregate any hard
carbon black lumps which may not have been thoroughly wet by the water.
9.10 Replace the sieve holder and sieve and wash for an additional 2 min.
9.11 Remove the sieve holder and sieve and dry for 1 h at 125°C.
9.12 Transfer the dried residue to a piece of smooth white bond paper and rub gently to remove any carbon black remaining
on the residue. Rub until the white paper no longer shows any smears.
NOTE 2—The purpose of gently rubbing the residue is to remove any black that may be clinging to the gritty residue. Do not apply excessive force
when rubbing, as this action may fracture the residue allowing it to escape, or may trap the residue in the paper causing a low grit determination. Similarly,
do not wear gloves when performing this step as the residue may be trapped in the glove material, giving a low result.
9.13 Brush all the loose residue to a tared weighing dish and weigh to the nearest 0.1 mg using the analytical balance.
10. Report
10.1 Report the following information:
10.1.1 Proper identification of the sample,
10.1.2 Identification of the sieve number, and
10.1.3 Result of the determinations reported to the nearest mg/kg (ppm).
11. Precision and Bias
11.1 These precision statements have been prepared in accordance with Practice D 4483. Refer to this practice for terminology
and other statistical details.
11.2 The precision results in this precision and bias section give an estimate of the precision of this test method with the
materials used in the particular interlaboratory program described below. The precision parameters should not be used for
acceptance or rejection testing of any group of materials without documentation that they are applicable to those particular
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D 1514 – 001
TABLE 1 Test Method D 1514 Test Method Precision—Type 1 (Sieve Residue Using a No. 325 Sieve)A
Material
B
A
C
Average
Pooled values
Within LaboratoriesB
Mean Level,
mg/kg (ppm)
9.3
52.9
137.0
66.4
Between LaboratoriesB
Sr
r
((r))
SR
R
2.62
8.02
19.16
7.42
22.70
54.22
79.5
42.9
39.6
7.09
28.79
42.29
20.08
81.49
119.68
12.09
34.20
51.5
29.82
84.39
((R))
215
154
87.3
127
A
This is short-term precision (days) with outliers removed from the data set.
B
Symbols are defined as follows:
Sr
r
(
(r))
SR
R
(R)
= within-laboratory standard deviation,
= repeatability (in measurement units),
= repeatability (in percent),
= between-laboratory standard deviation,
= reproducibility (in measurement units), and
= reproducibility (in percent).
materials and the specific testing protocols of the test method. Any appropriate value may be used from Table 2. A type 1
inter-laboratory precision program was conducted as detailed in Table 3. Both repeatability and reproducibility represent short term
(daily) testing conditions. The testing was performed using two operators in each laboratory performing the test once on each of
two days (total of four tests). A test result is the value obtained from a single determination. Acceptable difference values were not
measured. The between operator component of variation is included in the calculated values for (r) and (R).
11.3 The results of the precision calculations for this test are given in Table 2. The materials are arranged in ascending “mean
level” order.
11.4 Repeatability—The pooled relative repeatability, (r), of this test has been established as 80.8 %. Any other value in Table
2 may be used as an estimate of repeatability, as appropriate. The difference between two single test results (or determinations)
found on identical test material under the repeatability conditions prescribed for this test will exceed the repeatability on an average
of not more than once in 20 cases in the normal and correct operation of the method. Two single test results that differ by more
than the appropriate value from Table 2 must be suspected of being from different populations and some appropriate action taken.
NOTE 3—Appropriate action may be an investigation of the test method procedure or apparatus for faulty operation or the declaration of a significant
difference in the two materials, samples, etc., and so forth, which generated the two test results.
11.5 Reproducibility—The pooled relative reproducibility, (R), of this test has been established as 180 %. Any other value in
Table 2 may be used as an estimate of reproducibility, as appropriate. The difference between two single and independent test
results found by two operators working under the prescribed reproducibility conditions in different laboratories on identical test
material will exceed the reproducibility on an average of not more than once in 20 cases in the normal and correct operation of
the method. Two single test results produced in different laboratories that differ by more than the appropriate value from Table 2
must be suspected of being from different populations and some appropriate investigative or technical/commercial action taken.
11.6 Bias—In test method terminology, bias is the difference between an average test value and the reference (true) test property
value. Reference values do not exist for this test method since the value or level of the test property is exclusively defined by the
test method. Bias, therefore, cannot be determined.
12. Keywords
12.1 carbon black; non-carbon black residue; sieve residue; water wash sieve residue
TABLE 2 Precision Parameters for D 1514 Sieve Residue, (Type 1
(No. 325 Sieve) Precision)
Units
mg/kg (ppm)
Material
Mean Level
IRB#6 (N330)
N762
SRB A5 (N135)
N550
N650
Average
Pooled Values
18.3
18.3
20.8
64.3
75.7
39.5
4
Sr
(r)
SR
(R)
6.0
7.4
5.1
10.4
20.2
93.3
114
69.5
45.9
75.6
13.1
9.7
9.7
24.7
46.7
203
150
132
109
174
11.3
80.8
25.1
180
D 1514 – 001
TABLE 3 Interlaboratory Precision Program
Nominal Test Period
Material
March 1996
October 1996
March 1997
September 1997
March 1998
N650
IRB#6 (N330)
N762
SRB A5 (N135)
N550
Number of Laboratories
49
41
45
42
47
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